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IS 18130 : 2023
भारतीय मानक
Indian Standard

रोटरी वाष्पीकरण का उपयोग कर िवलयन

से कोलतार क� �रकवरी के िलए िविध

Method for Recovery of Bitumen

from Solution Using Rotary
Evaporator

ICS 91.100.50; 93.080.20

BIS 2023

भारतीय मानक ब्यरू ो

BUREAU OF INDIAN STANDARDS
मानक भवन, 9 बहादरु शाह ज़फर मागर्, नई िदल्ली - 110002
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI - 110002
www.bis.gov.in www.standardsbis.in

February 2023 Price Group 4

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Bitumen, Tar and Related Products Sectional Committee, PCD 6

FOREWORD
This Indian Standard was adopted by the Bureau of Indian Standards after the draft finalized by the Bitumen, Tar
and Related Products Sectional Committee had been approved by the Petroleum, Coal and Related Product
Division Council.
To determine the characteristics of the bitumen in a bitumen paving mixture, it is necessary to extract the bitumen
from the aggregate by means of a suitable solvent and then to recover the bitumen from the solvent without
significantly changing the bitumen properties. The bitumen recovered from the solvent by method can be tested
using the same methods as for the original bitumen and comparisons between the properties of the original and
recovered bitumen can bemade. It is also used to study the properties of bitumen aged in service.

When the bitumen is extracted from bituminous mixture by centrifuge method, some ultra-finemineral material
which passed through the filter may be present in the extract liquid. If the amount of this mineral material is more
than 1 percent, the properties of bitumen recovered by this method may be affected. In such cases, it is recommended
to remove the ultra- fine material from the extract liquid by using any suitable high-speed (3000 rpm or higher)
centrifuge of the continuous flow type.

Considerable assistance has been drawn from the ASTM D 5404-12 ‘Standard practice for recovery of asphalt
from solution using the rotary evaporator’ in formulation of this draft standard.

The composition of the Committee, responsible for formulation of this standard is listed in Annex A.

For the purpose of deciding whether a particular requirement of this standard is complied with the final value,
observed or calculated, expressing the result of a test or analysis shall be rounded off in accordance with
IS 2 : 2022 ‘Rules for rounding off numerical values (second revision)’. The number of significant places retained
in the rounded off value should be the same as that of the specified value in this standard.
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Indian Standard
METHOD FOR RECOVERY OF BITUMEN FROM SOLUTION
USING ROTARY EVAPORATOR

1 SCOPE
This standard prescribes the method of recovery of
bitumen from a solution using rotary evaporator
ensuring that changes in the bitumen properties
during recovery process are minimized.
2 REFERENCE
The following standards contain provisions which,
through reference in text constitute provisions of this
standard. At the time of publication, the editions
indicated were valid. All the standards are subject to
revision, and parties to agreements based on this
standard are encouraged to investigate the possibility
of applying the most recent editions of the standards
indicated below:
IS No. Title
IS 334 : 2002 Glossary of terms relating to
bitumen and tar (third revision)
3 TERMINOLOGY
For the purpose of this standard, the definitions
given in IS 334 shall apply.
4 PRINCIPLE
The solution of bitumen and solvent from a prior
extraction is distilled by partially immersing the
rotating distillation flask of the rotary evaporator
in a heated oil bath. The solution is subjected to
a partial vacuum and a flow of nitrogen gas or
carbon dioxide gas. These gases provide inert
atmosphere to prevent oxidation of the bitumen
during the recovery process.
NOTE — The quality of the results obtained from this
standard method are largely dependent on the competence
of the personnel performing the test and
calibration/maintenance of the test equipment.
5 APPARATUS
5.1 Rotary Evaporator — Equipped with a
distillation flask, a variable speed motor capable of
rotating the distillation flask (2 l capacity) at a rate
of about 50 rpm, condenser solvent recovery flask,
and heated oil bath. Angle of the distillation flask
from the horizontal to the bath is set at about 15° (see
Fig.1). The distillation flask when fully immersed,
should be at a depth of about 40 mm.

FIG. 1 ROTARY EVAPORATOR AND RECOVERY SYSTEM

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5.2 Thermometric Device — A built in temperature
measurement device capable displaying the oil
temperature to the nearest 1°C.
5.3 Manometer or vacuum gauge — Suitable for
measuring the specified vacuum (see cl. 7)
5.4 Gas flowmeter — Capable of indicating a gas
flow of up to 1000 ml/min.
5.5 Sample container — Having adequate volume
to hold the sample and added solvent.
5.6 Vacuum system — Capable of maintaining a
vacuum to within ± 0.7 kPa (± 5 mm of Hg) of the
desired level up to and including 80 kPa [600 mm of
Hg].
5.7 Oven — Capable of maintaining a temperature
of 165 °C ± 5 °C.
6 REAGENTS AND MATERIALS
6.1 Nitrogen Gas or Carbon Dioxide Gas — A
pressurized tank with pressure-reducing valve, or
any other convenient source.
NOTE — Different flow rates may be required whether
nitrogen gas or carbon dioxide gas is used.
6.2 Oil — The oil for the heated oil bath should be
food grade white oil or silicone fluid with flash point
above 215°C or an equivalent.
6.3 Solvents — The solvent for extracting the
bitumen from mixtures should be reagent grade
trichloroethylene or methylene chloride. It is
recommended that for each new supply of solvent,a
blank should be run on a bitumen with known
properties.
6.3.1 Precautions
6.3.1.1 The solvents listed in 6.3 should be used only
under a hood or with an effective surface exhaust
system exhaust system in a well-ventilated area, since
they are toxic to various degrees.
6.3.1.2 These solvents may be hydrolyzed in the
presence of heat and moisture to form acids that are
extremely corrosive to certain metals, especially
when subject to contact over lengthy periods to time.
It is necessary to take proper precautions to not allow
these solvents to remain in small quantities in the
effluent tanks of aluminum vacuum extractors.
6.3.1.3 Exposure of these solvents or their vapors to
high temperature such as contact with flames, hot
glowing surfaces, or electric arcs can produce
decomposition products such as hydrogen chloride.
Steel drums containing these solvents should be
stored in a cool, dry locations, kept tightly sealed,
and opened as infrequently as possible. The
hydrogen chloride in decomposed solvent may
harden a bitumen during the extraction and recovery
test and thusgive erroneous test results.
2
7 PROCEDURE
7.1 Heat the oil bath to temperature of 140 °C
± 3 °C. Start circulating cold water through
the condenser.
7.2 Apply a vacuum of 5.3 kPa ± 0.7 kPa
[40 mm Hg ± 5 mm Hg] below atmospheric
pressure and draw approximately 600 ml of
bitumen solution from the sample container into
the distillation flask through the sample line. Begin
a nitrogen or carbon dioxide flow of
approximately 500 ml/min through the system
(see Note). Begin rotating the distillation flask (at
approximately 40 rpm) and lower the flask into the
oil bath. Initially the immersion depth of the flask
will be determined by the need to achieve a
controlled solvent evaporation rate. The correct rate
of evaporation can be observed as steady
controlled stream of condensed solvent being
collectedin the recovery flask.
NOTE — The vacuum and nitrogen or carbon dioxide flow
values may need to be adjusted depending on thelocation.
Also, low flow values are recommended at the beginning of
the rotary process when the sample volume is large because
of the possibility of back flow into the vacuum system. The
possibility of back flow can also be minimized by regulating
the depth of immersion of the flask.
7.3 When the amount of bitumen solution within the
distillation flask appears low enough so that more
solution may be added, discontinue the nitrogen or
carbon dioxide flow. Draw the remaining bitumen
solution from the sample container into the
distillation flask and readjust the nitrogen or carbon
dioxide flow (see Note).
NOTE — The equipment may be modified to allow a
continuous flow of solution from the sample container into
the distillation flask such that the volume in the distillation
flask maintained at approximately 600 ml. The nitrogen or
carbon dioxide flow is not started until all the solution has
entered the distillation flask.
7.4 When most of the solvent has been distilled from
the bitumen and no obvious condensation is
occurring on the condenser, the flask should be
immersed to the recommended maximum
immersion depth of approximately 40 mm. Slowly
apply a vacuum of 80.0 kPa ± 0.7 kPa (600 mm of
Hg ± 5 mm of Hg) below atmospheric pressure.
Increase nitrogen or carbon dioxide flow to
approximately 600 ml/min and the spin rate of the
distillation flask to about 45 rpm. Hold or reduce
vacuum if foaming or a bubbly formation occurs.
When foaming subsides apply maximum vacuum.
Maintain this condition for 10 min ± 1 min.
NOTES
1 It is recommended that the flask be immersed for up to 2
min before slowly applying the vacuum.
2 A faster flask spin rate exposes more surface area of the
bitumen and, hence, dislodges more traces of solvent from
the bitumen. The rotation speed of the flask may also be
varied or flask rotation may be stopped to enhance the
removal of solvent.
3 Due to the cooling effect of the increased nitrogen or
carbon dioxide flow, an increase in the temperature of the
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oil bath is generally needed to maintain a constant sample
temperature. Experience has shown that a typical oil bath
temperature range of 150 °C to 155 °C is satisfactory for
this purpose.
7.5 At the end of the 15 min period, remove the
distillation flask from the apparatus and wipe the
flask to clean the oil. Pour the bitumen into a proper
size container. If needed, the flask may beinverted
and placed into an oven at 165 °C ± 1 °C for 10 min
to 15 min to cause the bitumen to flow into the
container. The bitumen should not be allowed to be
distributed over the interior of the flask.
7.6 Portions of the recovered bitumen, while still in
a liquid state, can be taken for determination of
properties such as penetration, viscosity, softening
point, ductility, Complex shear modulus G, and
angle as required.

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ANNEX A
(Foreword)
COMMITTEE COMPOSITION
Bitumen, Tar and Related Products sectional committee, PCD 6

Organization Representative(s)
CSIR — Central Road Research Institute, New Delhi DR AMBIKA BEHL (Chairperson)
Airports Authority of India, New Delhi SHRI VINOD KUMAR SHARMA
SHRI SUPRIO GOSH (Alternate)
Bharat Petroleum Corporation Limited, Mumbai SHRI C. SHANMUGANATHAN
MS SONAL MAHESHWARI (Alternate)
Birla Institute of Technology and Science, Pilani SHRI SRIDHAR RAJU
CSIR — Central Road Research Institute, New Delhi DR SIKSHA SWAROOP KAR
CSIR — North East Institute of Science and Technology, DR SHASHI D. BARUAH
Jorhat DR B. P. BARUAH (Alternate)
Central Public Works Department, New Delhi SHRI DIVAKAR AGRAWAL
Chennai Petroleum Corporation Limited, Chennai DR V. SELVAVATHI
SHRI H. RAMAKRISHNAN (Alternate)
Dilip Buildcon Limited, Bhopal SHRI B.B. KAMESWARA RAO
SHRI ANUSH K.C. (Alternate)
Directorate General Border Roads, New Delhi LT COL NITIN CHANDRA JOSHI
SHRI ARNAB CHAKRABORTY (Alternate)
Directorate General of Quality Assurance, Ministry of SHRI VIVEKANAND
Defence, New Delhi SHRI ANIL KUMBHARE (Alternate I)
SHRI SACHIN VINAYAK ZOPE (Alternate II)
Engineer in Chief Branch, New Delhi SHRI R. JAYAPRASAD
SHRI O P SRIVATAVA (Alternate)
G R Infra-Projects Limited, Gurugram SHRI U.C. GUPTA
GP Global Asphalt Private Limited, New Delhi SHRI RAJESH KUMAR JAIN
Highways Research Station, Chennai MS ER S. USHA DEVI
SHRI ER S. YAMINI (Alternate)
Hindalco Industries Limited, Mumbai SHRI HARSHAD KUMAR PANDIT
Hindustan Colas Private Limited, Mumbai SHRI T. K. SUBHAASH
SHRI K. G. RANGANATHA (Alternate)
Hindustan Petroleum Corporation Limited (HP Green R & D SHRI B. RAVI
Center), Bengaluru SHRI K. RAGHAVA KRISHNA (Alternate)
Hindustan Petroleum Corporation Limited, Mumbai SHRI SANTOSH DHAKU BHOGALE
IRB Infrastructure Developers Limited, Mumbai SHRI SUDHIR HOSHING
SHRI JITENDER CHAUHAN (Alternate I)
MS SONALI SARKAR (Alternate II)
Indian Institute of Petroleum, Dehradun SHRI MANOJ SRIVASTAVA
DR KAMAL KUMAR (Alternate)
Indian Institute of Technology Bombay, Mumbai DR DHARAMVEER SINGH
Indian Institute of Technology Delhi, New Delhi SHRI ARAVIND SWAMY

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IS 18130

Indian Institute of Technology Madras, Chennai DR J. MURALI KRISHNAN

DR A.VEERARAGHAVAN (Alternate)
Indian Institute of Technology, Roorkee SHRI SHAM SUNDAR RAVINDRANATH
Indian Oil Corporation Limited — Refineries and Pipelines SHRI S. SARKA
Division, New Delhi SHRI K. MEDHI (Alternate I)
DR MONIKA (Alternate II)
Indian Oil Corporation Limited, New Delhi DR N. S. RAMAN
Indian Road Congress, New Delhi SHRI S. K. NIRMAL
SHRI R. V. PATIL (Alternate)
Indian Oil Total Private Limited, Mumbai SHRI PANKAJ KUMAR JAIN
SHRI GAURAV GOGNE
Ministry of Road Transport and Highways, New Delhi SHRI SANJEEV KUMAR
SHRI VARUN AGGARWAL (Alternate)
National Institute of Technology, Warangal SHRI VENKAIAH CHOWDARY
DR S. SHANKAR (Alternate)
National Rural Roads Development Agency, New Delhi SHRI B.C. PRADHAN
National Test House, Kolkata SHRI VINAY KUMAR
Nayara Energy Limited, Mumbai SHRI MRIGANKA TARAFDAR
SHRI DHIRAJ GONDALIA (Alternate)
Om Infracon Private Limited, Guwahati SHRI A. N. DAS
Ooms Polymer Modified Bitumen Private Limited, Gurugram SHRI B.R. TYAGI
SHRI PALASH KATHAL (Alternate)
Shell Bitumen India Private Limited, Gurgaon SHRI NILANJAN SARKER
ZYDEX INDUSTRIES LIMITED SHRI AJAY RANKA
SHRI VISHAL SALUJA (Alternate I)
SHRI HIMANSHU AGARWAL (Alternate II)
Director General, BIS SHRIMATI MEENAL PASSI, SCIENTIST ‘F’/SENIOR DIRECTOR
AND HEAD (PETROLEUM, COAL AND RELATED PRODUCTS)
[REPRESENTING DIRECTOR GENERAL (Ex-officio)]

Member Secretary
SHRI HARI MOHAN MEENA
SCIENTIST ‘C’/DEPUTY DIRECTOR,
(PETROLEUM, COAL AND RELATED PRODUCTS)BIS

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development of the activities of standardization, marking and quality certification of goods and attending to
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This Indian Standard has been developed from Doc No.: PCD 06 (15409).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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